纳米 SiO 2/ LiClO 4/ PVDF2 HFP复合凝胶聚合物电解质的制备及其电化学性能

为了解决液态电解质锂离子电池存在的安全性问题 , 以偏氟乙烯和六氟丙烯的共聚物( PVDF2 HFP)为基体 , 通过加入高氯酸锂(LiClO 4) 、 增塑剂(碳酸丙烯酯和碳酸二甲酯) 、 纳米二氧化硅等 , 制备出了具有高电导率的复合凝胶聚合物电解质。用 X射线衍射仪测试聚合物电解质的结构 , 用交流阻抗法测定其电导率 , 用线性伏安扫描法研究了该聚合物电解质体系的电化学稳定性 , 并以其为电解质制备成锂离子电池进行充放电测试。结果- 3表明 , 在 20℃ 时复合凝胶聚合物电解质的电导率最高可达 7. 56×10 S/ cm , 该电解质在 41 6 V 以下电化学窗口稳定 , 以其为电解质的锂离子电池具有良好的电化学性能 , 说明纳米 SiO 2/ LiClO 4/ PVDF2 HFP复合凝胶聚合物电解质能满足锂离子电池的应用。     

纳米SiO2/LiClO4/PVDF-HFP复合凝胶聚合物电解质的制备及其电化学性能

为了解决液态电解质锂离子电池存在的安全性问题,以偏氟乙烯和六氟丙烯的共聚物(PVDF-HFP)为基体,通过加入高氯酸锂(LiC1O4)、增塑剂(碳酸丙烯酯和碳酸二甲酯)、纳米二氧化硅等,制备出了具有高电导率的复合凝胶聚合物电解质.用X射线衍射仪测试聚合物电解质的结构,用交流阻抗法测定其电导率,用线性伏安扫描法研究了该聚合物电解质体系的电化学稳定性,并以其为电解质制备成锂离子电池进行充放电测试.结果表明,在20℃时复合凝胶聚合物电解质的电导率最高可达7.56×10-3S/cm,该电解质在4.6 V以下电化学窗口稳定,以其为电解质的锂离子电池具有良好的电化学性能,说明纳米SiO2/LiC1O4/PVDF-HFP复合凝胶聚合物电解质能满足锂离子电池的应用.     

溶胶-凝胶法低温制备SrCe0.85Er0.15O3-α及其复合电解质的中温燃料电池性能

以溶胶-凝胶法低温(1 100℃)制备SrCe_(0.85)Er_(0.15)O_(3-α),并与NaCl-KCl共熔体进行复合,热处理温度(750℃)远低于通常高温烧结温度(1 500℃)。XRD结果表明NaCl、KCl与SrCe_(0.85)Er_(0.15)O_(3-α)复合后没有发生化学反应。采用电化学工作站研究了复合电解质在500~700℃下干燥氮气气氛中的电导率。结果表明,温度为700℃时,复合电解质在干燥氮气气氛中的电导率达到最大值1.1×10-1 S·cm-1,远高于单一铈酸锶材料在相同条件下的电导率。H2/O2燃料电池性能测试表明复合电解质在700℃最大输出功率密度为260.8mW·cm-2。     

硅酸盐氧基磷灰石的溶胶凝胶法制备与表征

为了提高电导率,以溶胶-凝胶法制备了硅酸盐氧基磷灰石.通过TG-DTA、XRD和IR分析,研究了从凝胶转变为硅酸盐氧基磷灰石过程中凝胶焙烧温度的影响.结果表明,制备Sr2La8(SiO4)6O2、La9.33(SiO4)6O2和La10(SiO4)6O3时凝胶的焙烧温度分别为850、950℃和950℃;间隙氧可能诱发晶体结构扭曲,晶胞体积变大.通过IR和XRD分析,证实了在La9.33(SiO4)6O2和La10(SiO4)6O3磷灰石中间隙氧的存在.     

杂多酸掺杂聚酰亚胺/二氧化硅复合质子交换膜的制备和性能研究

采用溶胶-凝胶法制备了杂多酸掺杂聚酰亚胺／二氧化硅（PI／SiO2）复合质子交换膜,研究了其质子导电性能、保水能力和抗化学氧化性能。结果表明,该千态复合膜的室温质子电导率为10^-7S／cm,中温环境（100～200℃）下的电导率可达10^-5S／cm以上,随着温度和杂多酸含量的升高,其质子电导率相应升高;对膜保水性能的研究表明,SiO2和杂多酸的加入能有效提高中温条件下复合膜的保水率,少量水的参与有可能进一步提高膜的质子电导率;对膜抗氧化性的研究表明,复合膜的抗氧化能力随二氧化硅含量的增加而增加,而随杂多酸含量的增加而降低,与纯聚合物相比,该复合膜的抗氧化能力略有下降。     

Ce1-xPrxO2-x/2的溶胶-凝胶法的合成及其性质

利用溶胶—凝胶法合成了Ce1-xPrxO2-x/2(x＝0—0．3)系列固体电解质，系统地研究了其结构和导电性。由于洛胶—凝胶法合成的物质粒度均匀，颗粒小，故在较低温度(1300℃)时即可形成高致密度样品。XPS测试表明掺杂后吸附氖浓度明显增大，氧空位增多，电导率和氧离子迁移数增大，改善了CeO2基固体电解质的性能。阻抗谱分析发现，在低温区电导率主要取决于晶界电导，而在高温区电导率主要取决于晶粒电导。     

SiO_2溶胶含量对Al_2O_3-SiO_2-TiO_2复合膜的影响

采用不同配比的Al2O3、SiO2、TiO2溶胶,通过溶胶-凝胶法制备Al2O3-SiO2-TiO2复合膜.通过凝胶时间、TG-DTG、FT-IR和AFM等表征手段对溶胶的稳定性、复合膜的热稳定性、结构特征和表面微观形貌进行综合分析.实验结果表明:SiO2溶胶含量是影响复合溶胶稳定性的主要因素,随着SiO2溶胶含量的增加,复合溶胶的稳定性越小,凝胶时间越短,制膜时间缩短;TG-DTG分析表明,350℃以后,无明显的热效应,可见三组分复合的膜热稳定性较好;FT-IR表明,整个复合体系是以Si-O-Si为主要支架结构的,并生成了更加稳定的氧桥键(Si-O-Al和Ti-O-Al-O-Si等)而形成网络结构;AFM分析表明,复合膜的孔隙率较高,具有纳米尺寸孔洞,5μm范围内膜表面不太平整,通过多次涂膜可以减小缺陷,平均孔径约为53.8nm.     

聚氨酯/SiO_2复合凝胶聚合物电解质的制备与性能EI北大核心CSCD

将聚氨酯(PU)与纳米SiO_2复合,采用相转移法制备了不同SiO_2含量的PU/SiO_2复合凝胶聚合物电解质。材料微观结构、热性能和电化学性能等测试结果表明,相转移法得到了多孔结构的聚合物膜,SiO_2颗粒较均匀地分散于PU基体中;随着SiO_2含量逐渐增加,电解质的吸液率和拉伸强度呈先上升后下降的趋势;差示扫描量热分析和热重分析测试结果表明,复合多孔电解质膜的玻璃化转变温度和热分解温度较纯PU有明显提高;SiO_2质量分数为5%时制备的PU/SiO_2复合多孔凝胶聚合物电解质综合性能最优,吸液率为163%,拉伸强度为5.45 MPa,5%分解温度高达324℃,20℃时离子电导率为3.02×10-3S/cm,电化学稳定窗口为5.32 V,显示了较好的应用前景。     

聚氨酯/SiO_2复合凝胶聚合物电解质的制备与性能

将聚氨酯(PU)与纳米SiO_2复合,采用相转移法制备了不同SiO_2含量的PU/SiO_2复合凝胶聚合物电解质。材料微观结构、热性能和电化学性能等测试结果表明,相转移法得到了多孔结构的聚合物膜,SiO_2颗粒较均匀地分散于PU基体中;随着SiO_2含量逐渐增加,电解质的吸液率和拉伸强度呈先上升后下降的趋势;差示扫描量热分析和热重分析测试结果表明,复合多孔电解质膜的玻璃化转变温度和热分解温度较纯PU有明显提高;SiO_2质量分数为5%时制备的PU/SiO_2复合多孔凝胶聚合物电解质综合性能最优,吸液率为163%,拉伸强度为5.45 MPa,5%分解温度高达324℃,20℃时离子电导率为3.02×10-3S/cm,电化学稳定窗口为5.32 V,显示了较好的应用前景。     

染料敏化太阳电池有序介孔SiO2/离子液体凝胶电解质的研究

以P123为模板剂,采用溶胶-凝胶法制备有序介孔SiO2,用N2吸附、扫描电镜及透射电镜对样品进行分析.结果表明,制备的介孔SiO2呈短棒状,具有有序柱状孔结构,平均孔径为5.75nm.有序介孔SiO2固化二元离子液体(1-甲基-丙基咪唑碘/1-甲基-己基咪唑碘)形成凝胶电解质.由于凝胶电解质中离子液体在介孔SiO2的孔道中有序排列,使凝胶电解质I3-的扩散系数增大,从而降低了电解质的内阻,抑制了染料敏化纳晶多孔膜-凝胶电解质界面的复合反应,使凝胶电解质染料敏化太阳电池具有较大的开路电压和填充因子,光电转换效率达到5.22%.     

Modified solid-state reaction synthesized cathode lithium iron phosphate (LiFePO4) from different phosphate sources

A modified solid-state method was used to prepare LiFePO4. With the aid of deionized water, a mixture containing Fe2O3, NH4H2PO4 (or (NH4)2HPO4), LiOH, glucose and oxalic acid was prepared into fluffy powders, which were heated in a carbon-coated crucible at 700 degrees C for 3 hours to synthesize LiFePO4 without any inert gas flow. For the first time, the roles of NH4H2PO4 and (NH4)2HPO4 on the preparation of LiFePO4 were systematically investigated. The obtained samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS), revealing that the crystallinity of the LiFePO4 sample prepared from NH4H2PO4 is superior to that prepared from (NH4)2HPO4 and the particle size of the sample prepared from NH4H2PO4 is smaller than that prepared from (NH4)2HPO4. The specific capacity, cycle property and rate capabilities were also compared between the as-prepared LiFePO4 samples. A better electrochemical performance was observed in the sample prepared from NH4H2PO4.     

溶胶凝胶法制备磷酸锆钠陶瓷材料

以Zr(NO3)4.5H2O、NH4H2PO4和NaNO3为原材料,采用溶胶凝胶法合成了磷酸锆钠(NaZr2(PO4)3)陶瓷粉体,采用TG-DTA,XRD和SEM测试方法对粉体性能进行了表征,研究了烧结温度和pH值等反应条件对粉体合成的影响.结果表明,要获纯的磷酸锆钠粉体,合成温度需控制在800～1 000℃之间,其中最合适合成温度为900℃左右.前驱体pH值对合成温度基本没有影响,但会影响产物微观形貌.当合成温度为900℃,pH值为9时可以制备出团聚较少、颗粒均匀、分散性较好且平均粒径为100nm的磷酸锆钠粉体.     

固体酸对介孔氧化铝导电性能影响

在介孔氧化铝(Al2O3)中掺杂固体酸硫酸氢铯(CsHSO4)制备具有高质子导电性能的材料.通过SEM、XRD表征其孔道形貌和晶型特点,采用氮吸脱附测试孔径大小和比表面积等性能参数,运用TG-DSC研究材料的热稳定性及水含量,并应用交流阻抗法测试材料导电率.结果表明,以仲丁醇铝为铝源,通过溶胶-凝胶法合成孔径约为25nm的介孔γ-Al2O3材料,材料具有介孔大小均匀、比表面积大、热稳定性高等特点;掺杂固体酸后,介孔Al2O3的导电率在低温范围提高一个数量级,热分析结果进一步证实固体酸的添加使介孔Al2O3的吸水率提高,从而使质子传导的速率增加,最终提高固体酸掺杂介孔Al2O3的导电率.     

pH值及含水量对自蔓燃制备TiO_2光催化性能的影响

为了考察pH值及含水量对溶胶-凝胶自蔓燃法制备TiO2粉体光催化性能的影响,以TiO(NO3)2为前驱体,在原料、燃烧剂和燃烧助剂的物质的量比为n(TiCl4)∶n(C6H8O7)∶n(NH4NO3)=1∶1∶3,以及煅烧温度550℃不变的情况下,改变溶胶pH值和含水量,制备TiO2粉体,利用X射线衍射和扫描电镜进行结构表征,通过降解亚甲基蓝验证光催化性能。结果表明:该条件下制备的TiO2粉体具有松散、多孔的特性,晶型为锐钛矿。在pH值为7、含水质量分数为50%的条件下,TiO2的光催化活性最高。     

Y2O3、Al2O3掺杂对CeO2的烧结及电性能的影响

本文采用溶胶-凝胶法制备了不同含量的Y2O3掺杂的CeO2粉体，并在4mol％Y2O3—CeO2粉体中掺入Al2O3，研究了各样品的烧结性能和电性能。结果表明：适量的掺杂Y2O3能提高氧化铈的密度，但Y2O3含量超过4％mol后密度下降。一定量的Al2O3也能提高材料的烧结密度。随着Y2O3含量的增大，CeO2的电导先增大后减小，而掺入Al2O3对材料的电导不利。     

Zeolite synthesis from paper sludge ash at low temperature (90 degrees C) with addition of diatomite

Paper sludge ash was partially converted into zeolites by reaction with 3M NaOH solution at 90 degrees C for 24 h. The paper sludge ash had a low abundance of Si and significant Ca content, due to the presence of calcite that was used as a paper filler. Diatomite was added to the NaOH solution to increase its Si content in order to synthesize zeolites with high cation exchange capacity. Diatomite residue was filtered from solution before addition of ash. The original ash without addition of diatomite yielded hydroxysodalite with a cation exchange capacity ca. 50 cmol/kg. Addition of Si to the solution yielded Na-P1 (zeolite-P) with a higher cation exchange capacity (ca. 130 cmol/kg). The observed concentrations of Si and Al in the solution during the reaction explain the crystallization of these two phases. The reaction products were tested for their capacity for PO(4)(3-) removal from solution as a function of Ca(2+) content, suggesting the formation of an insoluble Ca-phosphate salt. The product with Na-P1 exhibits the ability to remove NH(4)(+) as well as PO(4)(3-) from solution in concentrations sufficient for application in water purification. Both NH(4)(+) and PO(4)(3-) removal showed little variation with pH between 5 and 9. Alternative processing methods of zeolite synthesis, including the addition of ash to an unfiltered Si-NaOH solution and addition of a dry ash/diatomite mixture to NaOH solution, were tested. The third process yielded materials with lower cation exchange capacity due to formation of hydroxysodalite. The second process results in a product with relatively high cation exchange capacity, and reduces the number of processing steps necessary for zeolite synthesis.     

SrBi_4Ti_4O_(15)陶瓷材料介电和导热性能的研究

用溶胶-凝胶法制备了SrBi_4Ti_4O_(15)陶瓷材料,研究了烧结温度、铋含量及掺杂Nd对SrBi_4Ti_4O_(15)陶瓷结构、热扩散率及介电性能的影响.结果发现,SrBi_4Ti_4O_(15)陶瓷材料的热扩散率和介电常数随烧结温度的升高而增大,最佳烧结温度为1100℃,铋含量过量达10%时,SrBi_4Ti_4O_(15)陶瓷的热扩散率和介电常数最大.随着掺杂量Nd的增加,SrBi_4Ti_4O_(15)陶瓷的热扩散率和介电常数随之增大.     

尿素改性对钠离子电池负极材料NaTi_2(PO_4)_3电化学性能的影响

为提高水溶液钠离子电池负极材料NaTi_2(PO_4)_3(NTP)的导电性和倍率性能,以尿素(CO(NH_2)_2)为碳源采用溶剂热法合成了CO(NH_2)_2/NaTi_2(PO_4)_3(C/NTP)复合负极材料。采用XRD、SEM、TEM、Raman和恒流充放电等手段分析了材料的结构、C/NTP形貌和电化学性能。研究了不同阶段升温速率对C含量、包覆层石墨化程度及对电化学性能的影响。实验结果表明,低于400℃升温速率越小,C/NTP残碳量越高;400~650℃之间升温速率越小,包覆层石墨化程度越高,并提高了其电化学性能;在5C倍率下2℃/min热处理的样品首圈放电比容量为114.9mAh·g~(-1),循环30次后容量保持在91.9mAh·g~(-1);10C下放电比容量为87mAh·g~(-1),20C下放电比容量仍保持在71mAh·g~(-1),展现出高倍率下优异的循环性能。     

Transport Properties of K_xV_2O_5·nH_2O Nanocrystalline Films

Five different compositions of K x V 2 O 5 ·nH 2 O(where x=0.00,0.0017,0.0049,0.0064 and 0.0091 mol) were prepared by the sol-gel process.Electrical conductivity and thermoelectric power were measured parallel to the substrate surface in the temperature range of 300-480 K.The electrical conductivity showed that all samples were semiconductors and that conductivity increased with increasing K content.The conductivity of the present system was primarily determined by hopping carrier mobility.The carrier density was evaluated as well.The conduction was confirmed to obey non-adiabatic small polaron hopping.The thermoelectric power or Seebeck effect,increased with increasing K ions content.The results obtained indicated that an n-type semiconducting behavior within the temperature range was investigated.     

Measurement of ammonia in human breath with a liquid-film conductivity sensor

Measurement of breath NH3 is of interest in clinical applications as it can be used as a measure of kidney/liver functions as well as halitosis. We have developed a liquid-film conductivity sensor to measure NH3 in human breath. A film of dilute H2SO4 is formed on the top of two metal capillary tubes placed in a concentric annular arrangement. The tube exterior has been specially treated to render it hydrophilic. As breath passes over the sensor tip, the film collects NH3 and the solution conductivity (measured by the concentric capillaries functioning as electrodes) decreases accordingly. This initial rate of conductivity decrease was determined to be the best metric (most rapid and least dependent on breath pCO2) for ammonia, relative to time to attain complete neutralization (conductivity minimum) or the final rate of conductivity increase as more ammonia dissolves after neutralization. The absorbing solution composition was optimized so that CO2 does not interfere. Both dynamic measurement using mask sampling and offline balloon sampling were performed. Ammonia readily absorbs on surfaces when significant concentrations of water vapor are present. As such, memory effects are common when analyzing human breath for ammonia. This problem was successfully eliminated. The results from this sensor agreed well with data obtained by a solution-phase fluorometric technique using a porous membrane diffusion scrubber and o-phthalaldehyde derivatization chemistry. For breath CO2 measurement, the applicability of a similar sensor that relies on a NaOH film was also demonstrated.